Hydrochloric Acid → Piperazic acid t-butyl ester dihydrochloride salt

HRID 542746

반응식

HRID 542746 반응식
S(=O)(=O)(O)O.[N:6]1([C:12]([OH:14])=[O:13])[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1.[CH3:15][C:16](=[CH2:18])[CH3:17].[OH-].[Na+].[ClH:21]>CCOCC.O1CCOCC1>[ClH:21].[ClH:21].[C:16]([O:13][C:12]([N:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1)=[O:14])([CH3:18])([CH3:17])[CH3:15]

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 1118Sulfuric AcidHCID 8255IsobutyleneHCID 14798Sodium HydroxideHCID 131766Piperazine-1-carboxylic acid

생성물 1

HCID 67206290Piperazic acid t-butyl ester dihydrochloride salt

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 312751,4-Dioxane용매

실험 절차

A 250 ml pyrex heavy-walled pressure bottle is charged with 50 ml of dioxane, 3 ml of concentrated sulfuric acid, 1.3 g (0.01 mole) of piperazic acid (II-A) and approximately 75 ml of isobutylene, liquified by passage into a large test-tube cooled in a dry ice-acetone bath. The bottle is closed with a rubber stopper, clamped securely in place, and is shaken mechanically at room temperature overnight. The bottle is chilled in an ice bath and opened. The contents are poured into a separatory funnel containing a cold mixture of 200 ml of ether and 125 ml of 1N sodium hydroxide. The aqueous layer is washed with ether. The combined ethereal solution is dried over sodium sulfate and evaporated under vacuum to afford an oil, which is dissolved in 25 ml of ether. Addition of dry hydrogen chloride gives 1.3 g of crystalline piperazic acid t-butyl ester dihydrochloride salt (II-B).

후처리

  1. customliquified by passage into a large test-tube
  2. temperaturecooled in a dry ice-acetone bath
  3. customThe bottle is closed with a rubber stopper
  4. temperatureThe bottle is chilled in an ice bath
  5. additionThe contents are poured into a separatory funnel
  6. additioncontaining
  7. washThe aqueous layer is washed with ether
  8. dry with materialThe combined ethereal solution is dried over sodium sulfate
  9. customevaporated under vacuum
  10. customto afford an oil, which

출처 및 근거

ORD 기록
ord-6e44bd37e4854f49b1d4695524679ea3
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659711

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